Application and Development Trends of Spectral Analysis in Draft of Non-Ferrous Metal Standards in China

Spectral analysis was a method of identifying substances, determining their chemical composition and calculating their content based on their spectral characteristics. This paper mainly discussed the application of various spectroscopic techniques, mainly including atomic absorption spectrometry (AAS) inductively coupled plasma emission spectrometry (ICP-AES) X-ray fluorescence spectroscopy (XRF) atomic fluorescence spectroscopy (AFS) direct reading spectroscopy (OES) glow discharge emission spectroscopy (GD-OSE) laser-induced breakdown spectroscopy (LIBS), in the formulation of non-ferrous metal standards in China. The AAS method was the most widely used single-element microanalysis method among the non-ferrous metal standards. The ICP-AES method was good at significant advantages in the simultaneous detection of multiple elements. The XRF method was increasingly used in the determination of primary and secondary trace elements due to its simple sample preparation and high efficiency. The AFS was mostly detected by single-element trace analysis. OES GD-OES and LIBS were playing an increasingly important role in the new demand area for non-ferrous metals. This paper discussed matrix elimination, sample digestion, sample preparation, instrument categories and other aspects of some standards, and summarized the advantages of spectral analysis and traditional chemical analysis methods. The new methods of future spectroscopic technology had been illustrated in the process of developing non-ferrous metal standards.

特征荧光X射线吸收法精确测定基于铍膜的^(235)U裂变靶厚度

研究发展了一种基于特征荧光X射线吸收谱的、可精确测量裂变物质质量厚度的方法,系统分析了测量不确定度。实验结果表明,该方法可有效测定基于铍膜的235U裂变靶质量厚度,测量不确定度小于5%,其不确定度主要来源于测量的统计性。

Analysis of nickel distribution by synchrotron radiation X-ray fluorescence in nickel-induced early- and late-phase allergic contact dermatitis in Hartley guinea pigs

Background: Nickel-induced allergic contact dermatitis (Ni-ACD) is a global health problem. More detailed knowledge on the skin uptake of haptens is required. This study aimed to investigate the penetration process and distribution of nickel in skin tissues with late phase and early phase of Ni-ACD to understand the mechanisms of metal allergy. Methods: Forty Hartley guinea pigs were divided into four groups according to the NiSO4 sensitizing concentration and the NiSO4 challenged concentration: the 5% NiSO4-group, 5% to 10%(sensitization-challenge;late phase group);10% NiSO4-group, 10% to 10%(sensitization-challenge;early-phase group);and the positive and negative controls. Pathological biopsies were performed on each group. The depth profile of nickel element concentration in the skin of guinea pigs was detected by synchrotron radiation micro X-ray fluorescence spectroscopy (SR-μ-XRF) and micro X-ray absorption near-edge spectroscopy (μ-XANES). Results: In each section, the nickel element concentration in both the 5% NiSO4-group and 10% NiSO4-group was significantly higher than that in the negative control group. In the upper 300-μm section of skin for the early phase group, the nickel element concentration was significantly higher than that in the lower section of skin. In deeper sections (>200 μm) of skin, the concentration of nickel in the early phase group was approximately equal to that in the late phase group. The curve of the late phase group was flat, which means that the nickel element concentration was distributed uniformly by SR-μ-XRF. According to the XANES data for the 10% NiSO4 metal salt solution, structural changes occurred in the skin model sample, indicating that nickel was not present in the Ni^2+ aqueous ionic state but in the nickel-binding protein. Conclusions: This study showed that the distribution of the nickel element concentration in ACD skin tissue was different between the early phase and late phase groups. The nickel element was not present in the Ni^2+ aqueous ionic state but bound with certain proteins to form a complex in the stratum corneum in ACD model tissue.

Development and Application of Portable Reference Radiation Fields with Multi-Point Single-Energy Photon

Based on the needs of detection and calibration with low-energy X-ray, we used the relationship characteristics of X-ray fluorescence, absorption and limit potential target excitation, developed the X-ray device with adjustable intensity (single photon to 107/s), optional energy points (4 keV - 20 keV), highly portable (≤1 kg), by the matching design of fluorescence energy conversion target and modulation means, coupled transport simulation of electron-photon in target, meanwhile, we solved the low-energy X-ray radiation field diagnose problems with HPGe detector, which calibrated with combined technique, including relatively wide energy efficiency simulation and single energy point of absolute efficiency calibration. In single-photon calibration field of soft X-ray pulsar navigation detect, the portable reference single energy radiation fields was applied effectively and got good result, the reference radiation fields provided perfect experiment means for the scientific study of pulsar navigation detecting, sun X-ray monitoring, etc.

喀斯特地区端元样品中溶解有机质的多维特征与源辨析研究

由于喀斯特地区水生生态系统中碳循环的复杂性,给溶解有机质(Dissolved organic matter,DOM)的来源解析带来了巨大的挑战和困难.本研究应用C/N比值、δC组成、紫外-可见吸收光谱与三维荧光光谱等表征技术,综合对比了西南喀斯特地区典型土壤与水生植物样品DOM的多维特征,探讨了示踪喀斯特地区DOM来源的可靠方法与指标.结果表明:水生植物的C/N比值波动范围较大,石灰土的C/N比值偏低,水生植物与土壤样品的C/N比值及δC组成有所重叠,难以区分DOM的来源.多种紫外吸收系数(a_(254)、a_(280)、a_(300)与a_(350))侧面反映了不同DOM样品中芳香族化合物的相对丰度,SUVA_(254)、E2/E3、E4/E6与腐殖化指数(HIX、HIXohno)指示了样品之间腐殖化程度的差异,特别是HIX、荧光指数(FI)、SR较好区分了浮游藻类与土壤DOM.修正荧光指数(YFI)还揭示了不同DOM样品的化学组成,与三维荧光光谱的平行因子分析相吻合.此外,黄壤因较低的pH值会使土壤有机质酸解为含氮组分,导致HIX、FI和SR的匹配性不好.除浮游藻类外,HIX表明水生植物DOM均为内源,SR却显示其主要为外源,而FI指示兼有内源和外源.因此,在进行喀斯特地区DOM来源解析时,光谱技术相比C/N比值和δC分析更加简便、有效,同时应注意不同土壤类型的异质性与水生生态系统的复杂性.

Foliar application of rare earth elements on soybean(Glycine max(L)):Effects on biometrics and characterization of phytotoxicity

This study aims at investigating the effects of foliar application of aqueous solutions of La3+and Ce3+nitrates on soybean plants(Glycine max).First,we observe that Triton HW 1000 surfactant at 0.01 vol%reduces droplets contact angle and increases their drying time.Under greenhouse conditions,the foliar treatments do not affect chlorophyll content,plant height,number of leaves,number of pods,number of seeds per pod,and average seed weight.However,the treatments induce phytotoxicity since foliar injuries appear after the spraying.Microprobe X-ray fluorescence spectroscopy combined to scanning electron microscopy shows that the leaf lesions are positively correlated to accumulation of Ce and La on the leaf surface and also promote structural alteration to the epidermal cells.X-ray absorption near edge structure shows that the La and Ce nitrates are partially bio transformed into oxides by the leaves which might explain the harmful effects.

Total electron yield mode for XANES measurements in the energy region of 2.1-6.0 keV

The total electron yield （TEY） mode has been developed successfully for XANES measurements at Beamline 4BTA of BSRF （Beijing Synchrotron Radiation Facility）. Its performance was studied by measuring sulphur K-edge XANES of three CdS samples （mixed with graphite powder as an electric conductor） with different concentration： 75%, 50~ and 25%. The data are collected in TEY mode and fluorescence yield （FY） mode respectively for comparison. The results demonstrate that the TEY spectra of three samples agree well with each other after the background is subtracted and normalized. The measured XANES spectra by TEY mode without bias and with 100V bias are almost identical to one another, but the signal-to-noise ratio of spectra measured without bias is better than that with 100V bias. The consistency of the self-absorption corrected FY spectra and TEY spectra are within 10% for the three samples.